Revisions to ASTM D7310 Standard Guide for Defect Detection and Rating of Plastic Films Using Optical Sensors

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1 Revisions to ASTM D7310 Standard Guide for Defect Detection and Rating of Plastic Films Using Optical Sensors ANTEC 2017 Brenda Colegrove, The Dow Chemical Company Richard Garner, Borealis Dow.com SPE ANTEC Anaheim 2017 / 1370

2 Participating Companies SPE ANTEC Anaheim 2017 /

3 Historical Perspective on ASTM Gel Standards ASTM D3351 Visual/projector ASTM D7310 Optical Imaging ASTM D3596 PVC visual/light box Test Method Issued 1993 Withdrawn 2000 Guide Issued 2007 Revised 2011 Practice Issued 1992 Revised 2001, 2009, 2013, 2014 Sample Prep Gel Definition Film Plastic nodule not blended with matrix Excludes foreign particles Flat or tubular extrusion Any entity large enough to be detected by an optical sensor ; polymer as well as foreign particles Formulated with stabilizer & carbon black Compression molded sheet conditions given Hard particle of resin which will not fuse when the plastic mass is subjected to set conditions of hot processing. Clear, unpigmented area. Gel Size & Precision m, > 800 m Counts per 1520 cm 2 (4 layers) Reporting Counts per 1520 cm 2 ( 100 m thickness) Per agreement between supplier and customer None Very different! A. >500 m, 1 B m, 5 C m, 12 Counts per 232 cm 2 (500 m thickness) SPE ANTEC Anaheim 2017 /

4 Evolution of an ASTM Measurement* Standards Specific General Goal for revision Guide Def - a compendium of information or series of options that does not recommend a specific course of action. ASTM D7310 Defect Detection and Rating of Plastic Films Using Optical Sensors Practice Def - a definitive set of instructions for performing one or more specific operations that does not produce a test result. E.g. application, assessment, cleaning, collection, decontamination, inspection, installation, preparation, sampling, screening, and training. ASTM D3596 Determination of Gels (Fisheyes) In General-Purpose Poly(Vinyl Chloride) (PVC) Resins Method Def - a definitive procedure that produces a specific test result. Precision and bias is reported (method capability) ASTM D3351 Gel Count of Plastic Film (Withdrawn) *Does not include Classification, Specification, Terminology, SPE ANTEC Anaheim 2017 /

5 Definitions Clarification of defect defect for the purpose of this practice any entity in the film that is large enough to be detected by an optical sensor and is either polymeric in nature or caused by degradation, external contamination, undispersed additives or pigments, or similar sources. The defects can be classified in to three groups: Gels- A particle of plastic material in the film matrix not blended with the matrix and often acts as a miniature lens Contaminations- Any particle in or on the film matrix making the film significantly less transparent in transmission mode films than the matrix, or.; in reflection mode ( dirt, insects, oxidized additives or material, catalyst residues, solid particles, metallic particles, undispersed pigments or additives, etc.) Structural defects- Visual deviations not caused by gels or contaminations, e.g. air bubbles, wrinkles, die lines, film holes shark skin, arrow heads. Typical examples (pictures) are included in a new appendix. SPE ANTEC Anaheim 2017 /

6 Added Definitions parcel a user defined smallest area of inspected film for statistical analysis to which a detected defect can be attributed. The statistical evaluation is based on number of parcels effective pixel size distance between adjacent, individual pixels (picture elements) in the analyzed image The effective pixel size of the optical system is determined by the physical pixel size of the sensor and a magnification factor resolution representing the optical smallest pixel that is used for object size calculation Optical resolution Smallest resolvable distance.= pixel size x 2.3 (area = 4 pixels) SPE ANTEC Anaheim 2017 /

7 Size Verification Procedure Calibration object A transparent plastic substrate printed with circular black points ranging in diameter from 100 to 3000 microns (certified by vendor or confirmed with optical microscopy). Place object on running film Capture image Compare measured diameters to certified values Determine resolution from known diameter and number of pixels Hardware calibration is performed by camera vendor SPE ANTEC Anaheim 2017 /

8 Workflow for New Material 1. Determine material properties, MI/MFR and density optionally DSC to determine T m and degradation temperature 2. Estimate extrusion temperature as follows (linear across zones): Die. T m C Feed. T m 10C 3. Evaluate suitability considering: Extruder pressure, temperature of melt, film thickness and visual quality 4. Adjust as necessary 5. Establish camera settings Set gray value at 2/3 of range Verify sizing accuracy using calibration object Measure response on a sample over range of sensitivity values. Optimum setting is where the response is stable. 6. Further optimize extruder settings SPE ANTEC Anaheim 2017 /

9 Reporting Requirements Standard Report Evaluation Method Detection System Sample identification Date of sample Method used Film thickness Inspection area Density, if number of defects/ m² is reported the density needs to be reported for possible recalculation Defect observation, type (if different types are defined) and size. Exclude any defects with a reported size below the size limit of detection established for the optical system, as defects of this size cannot be consistently detected by the system. Statistical interpretation Identification of instrumentation used Extruder line Type (Lab or Production scale); Cast or Blown; Continuously or batch fed Operating conditions for the material Description of the screw Description of the die Description of the take-of unit Description of the distance between die & chill roll, the angle of the film coming the chill roll, position of air knife Scanner Mode (Transmission or Reflection (and angles of camera and light source to the film for reflection)) Light source type, color, and orientation (diffuse or parallel) Effective pixel size Any test settings that establish the criteria for defining the defect area (e.g. Sensitivity, grey level, shape factor, use of any type of filters applied to eliminate detected defects) SPE ANTEC Anaheim 2017 /

10 Variables Impacting Reported Gel Results Continuous pellet feed from process Melt Extruder Extruder size and type Number of zones Screw geometry Die design Screen pack Temperature profile Extruder speed Purging /cleaning practices Pressure Motor load Output Temperature at die Residence time Moisture Foreign Contamination Additive agglomerates Temperature at feed throat Continuous or batch fed Chill Rolls Sticking Slippage Wrinkles Coating Temperature Speed Die to chill roll distance Air Knife Air flow Distance to chill roll Angle of orientation Light Fluorescent Halogen LED Color Camera Pixel resolution Gain Line vs. matrix CCD vs. CMOS Environment Ambient air quality (dust, fibers) Winder Speed Rubber banding Film thickness Film tension Hardware, Software/Operational, Dependent SPE ANTEC Anaheim 2017 /

11 Protocol for First Round Robin Participation was anonymous Sample selection : LDPE samples provided by six resin producers Equipment vendors selected 1 sample unknown to participating companies Material information provided: MFR and density Sample size: 25 kg standard neutral bag Inspected area: 10 m² per test Defined size classes and reporting units (counts/m2) Equipment used was exactly described in a form created by equipment vendors Use local cleaning procedure prior to testing sample SPE ANTEC Anaheim 2017 /

12 Learnings from First Round Robin No two equipment setups were identical. Differences in: Geometries of the screws, lengths of compression / metering are different Diameters are different 19/20/25/30 Distance between die and chill roll vary (2 mm to 47 mm) Temperature profiles were different Chill roll temperatures varied from C 2 companies with conflicting information related to die and screw Screw speeds Take off speed SPE ANTEC Anaheim 2017 /

13 Learnings from First Round Robin Non uniform reporting Large variability in settings Vocabulary not fully clear Film thickness varied (no correction applied) 3 labs excluded due to not enough data to compare 1 major outlier. Note: Only 2 m² area inspected Others fall into 2 groups (based on Counts >100µm) Driven by smallest gel class Groups depend on smallest size considered SPE ANTEC Anaheim 2017 /

14 Data Analysis 10,000 1, A B 10 1 A B 0 SPE ANTEC Anaheim 2017 /

15 Consensus on most important factors Based on RR data + shared experience Temperature of die and temperature profile of extruder Extruder torque and pressure Screw mixing elements Sensitivity + grey levels Chill roll (esp. small gels) + air knife settings Lighting source SPE ANTEC Anaheim 2017 /

16 Protocol for Second Round Robin Samples: LDPE, HDPE, PP Each provided by single supplier (2 x 25kg bags) 3 tests, each 10m 2 inspected area Defined thickness (50 m) Extrusion temperature profiles set by resin supplier Results reports as counts/m 2 in defined size classes Data analysis by ASTM is in progress. SPE ANTEC Anaheim 2017 /

17 Summary of Changes Limited by inclusion of resin (lab extruder) as well as film (commercial extruder) Definitions: Updated and added additional terms Added example pictures of common defects Considerations for calibration and verification Proposed a workflow to establish test conditions for unfamiliar materials Elaborated on minimum reporting requirements Precision statement in progress based on round robin including 3 materials (LDPE, HDPE, and PP) SPE ANTEC Anaheim 2017 /

18 Thank You SPE ANTEC Anaheim 2017 / 1387

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